公开(公告)号：US4588829A

公开(公告)日：1986-05-13

申请号：US635283

申请日：1984-07-27

申请人： Wie-Hin Pan ,  Edward I. Stiefel

发明人： Wie-Hin Pan ,  Edward I. Stiefel

IPC分类号： C07F11/00 ,  C10M135/18

CPC分类号： C10M135/18 ,  C07F11/005

摘要： This invention relates to (disulfido)tris(N,N-substituted dithiocarbamato)Mo(V) complexes. More particularly, this invention relates to compounds of the formula MoS.sub.2 (S.sub.2 CNR.sub.2).sub.3 which are mononuclear, eight-coordinate, neutral Mo(V) complexes containing only eight sulfur atoms in the Mo coordination sphere. R is hydrogen, an alkyl, aryl, cycloalkyl group or mixture thereof. Preferably all of the R's are the same and are alkyl groups. These compounds are useful as lubricant additives.

摘要翻译： 本发明涉及（二硫化物）三（N，N-取代二硫代氨基甲酰）钼（V）络合物。 更具体地说，本发明涉及式MoS2（S2CNR2）3的化合物，它们是在Mo配位球中仅含有8个硫原子的单核，8位，中性Mo（V）络合物。 R是氢，烷基，芳基，环烷基或其混合物。 优选地，所有的R都是相同的并且是烷基。 这些化合物可用作润滑剂添加剂。

公开(公告)号：US5300274A

公开(公告)日：1994-04-05

申请号：US603064

申请日：1990-10-25

申请人： Liwen Wei ,  Catherine L. Coyle ,  Thomas R. Halbert ,  Edward I. Stiefel

发明人： Liwen Wei ,  Catherine L. Coyle ,  Thomas R. Halbert ,  Edward I. Stiefel

IPC分类号： C01G39/00 ,  C07F11/00 ,  C01G39/06

CPC分类号： C07F11/005 ,  C01G39/006 ,  C01P2006/60 ,  C01P2006/80 ,  C01P2006/82 ,  Y10S423/14

摘要： A method for preparing molybdenum and sulfur containing compounds of the general formula X.sub.2 Mo.sub.2 S.sub.12.yH.sub.2 O, where X is a cation selected from the group consisting of Na.sup.+, K.sup.+, R.sub.4 N.sup.+, R.sub.3 NH.sup.+, R.sub.2 NH.sub.2.sup.+, RNH.sub.3.sup.+, NH.sub.4.sup.+, R.sub.4 P.sup.+, R.sub.4 As.sup.+,(R.sub.3 P).sub.2 N.sup.+, R is a C.sub.1 -C.sub.30 alkyl, C.sub.6 -C.sub.30 aryl, C.sub.7 -C.sub.30 aralkyl or C.sub.2 -C.sub.30 alkoxyalkyl group and mixtures thereof, and y is from 0 to 2. The method comprises preparing a sulfide solution that contains from about 9 wt. % to about 13 wt. % sulfide sulfur; contacting the solution with elemental sulfur and a hydroxide; adding a molybdenum compound for a time and at a temperature sufficient to form a reaction mixture and a precipitate; separating the precipitate; and contacting the remaining reaction mixture with additional sulfide solution to form (NH.sub.4 ).sub.2 Mo.sub.2 S.sub.12.yH.sub.2 O. When compounds containing cations other than NH.sub.4.sup.+ are to be produced, the (NH.sub.4).sub.2 Mo.sub.2 S.sub.12.yH.sub.2 O is contacted with a cation exchange compound containing a desired substitute cation selected from above and an anion selected from the group consisting of Cl.sup.-, Br.sup.-, F.sup.-, I.sup.-, BF.sub.4.sup.-, PF.sub.6.sup.-, OH.sup.-, BR.sub.4.sup.- where R is a C.sub.1 -C.sub.30 alkyl, C.sub.6 -C.sub.30 aryl, C.sub.7 -C.sub.30 aralkyl or C.sub.2 -C.sub.30 alkoxyalkyl group, and mixtures thereof, in the presence of a solvent and for a time and at a temperature sufficient to form X.sub.2 Mo.sub.2 S.sub.12.yH.sub.2 O, where X is other than NH.sub.4.sup.+.

摘要翻译： 一种制备通式为X2Mo2S12.yH2O的含钼和硫化合物的方法，其中X是选自Na +，K +，R4N +，R3NH +，R2NH2 +，RNH3 +，NH4 +，R4P +，R4As +，（R3P）2N + R为C1-C30烷基，C6-C30芳基，C7-C30芳烷基或C2-C30烷氧基烷基及其混合物，y为0至2.该方法包括制备含有约9wt。 ％至约13重量％ 硫化硫％ 使溶液与元素硫和氢氧化物接触; 在足以形成反应混合物和沉淀物的温度下加入钼化合物; 分离沉淀物; 并将剩余的反应混合物与另外的硫化物溶液接触以形成（NH 4）2 Mo 2 S 12·yH 2 O。 当要生产含有除NH4 +之外的阳离子的化合物时，（NH 4）2 Mo 2 S 12·yH 2 O与含有选自上述的所需取代阳离子的阳离子交换化合物和选自Cl-，Br-，F - ，I - ，BF4-，PF6-，OH-，BR4-，其中R是C1-C30烷基，C6-C30芳基，C7-C30芳烷基或C2-C30烷氧基烷基，及其混合物， 溶剂并在足以形成X2Mo2S12.yH2O的温度下进行，其中X不是NH 4 +。

公开(公告)号：US5099046A

公开(公告)日：1992-03-24

申请号：US703219

申请日：1991-05-20

申请人： Catherine L. Coyle ,  Peter J. Guzi ,  Thomas R. Halbert ,  Edward I. Stiefel

发明人： Catherine L. Coyle ,  Peter J. Guzi ,  Thomas R. Halbert ,  Edward I. Stiefel

IPC分类号： C07F11/00

CPC分类号： C07F11/005

摘要： The present invention provides an improved method for preparing compounds of the formula Mo.sub.4 S.sub.4 L.sub.6 comprising:contacting a compound having the formula Mo.sub.2 S.sub.4 L.sub.2, wherein L is a 1,1-dithioacid ligand, with a reducing agent having a reduction potential sufficient to reduce Mo(V) to lower oxidation states, especially to Mo(III) and Mo(IV), at a temperature and for a time sufficient to form the Mo.sub.4 S.sub.4 L.sub.6 compound. Preferably, the Mo.sub.2 S.sub.4 L.sub.2 compound is dissolved in an organic solvent along with the reducing agent and the solution is heated at temperatures above 25.degree. C., up to the boiling point of the solvent and, more preferably, at temperatures in the range of from about 50.degree. C. to about 250.degree. C.

摘要翻译： 本发明提供了一种制备式Mo4S4L6化合物的改进方法，其包括：使具有式Mo2S4L2的化合物（其中L为1,1-二硫酸配体）与还原剂接触，还原剂具有足以还原Mo（V） 在足以形成Mo4S4L6化合物的温度和时间下，降低氧化态，尤其是Mo（III）和Mo（IV）。 优选地，将Mo 2 S 4 L 2化合物与还原剂一起溶解在有机溶剂中，并将溶液在高于25℃的温度下加热至溶剂的沸点，更优选在约 50℃至约250℃

公开(公告)号：US4832877A

公开(公告)日：1989-05-23

申请号：US101674

申请日：1987-09-28

申请人： Avi Bino ,  David C. Johnston ,  Edward I. Stiefel

发明人： Avi Bino ,  David C. Johnston ,  Edward I. Stiefel

IPC分类号： C07F11/00

CPC分类号： C07F11/005

摘要： Broadly stated, the present invention encompasses tetranuclear sulfide-bridged complexes of Cr(III) having bridging organo-carboxylate ligands. Indeed, in one embodiment, the present invention is directed toward a novel composition of matter having a complex cation of the general formula Cr.sub.4 S(RCO.sub.2).sub.8 (L).sub.4.sup.2+, wherein R represents alkyl groups having from 1 to 12 carbon atoms, L represents a ligand or ligands containing a donor atom selected from oxygen, nitrogen, carbon, and sulfur. In the complex of the present invention, the four Cr(III) atoms are bound to a central tetrahedral sulfur atom. The chromium atoms also are octahedrally coordinated with bridging carboxylates and the ligand molecule. Also, the bridging carboxylates, RCO.sub.2 of the above formula, are the same or different carboxylates.

公开(公告)号：US4585882A

公开(公告)日：1986-04-29

申请号：US635282

申请日：1984-07-27

申请人： Edward I. Stiefel ,  Wie-Hin Pan ,  Thomas R. Halbert

发明人： Edward I. Stiefel ,  Wie-Hin Pan ,  Thomas R. Halbert

IPC分类号： B01J31/18 ,  B01J31/22 ,  C07F11/00

CPC分类号： C07F11/005 ,  B01J31/226 ,  B01J2531/66

摘要： This invention relates to sulfido(disulfido)bis(N,N-substituted dithiocarbamato)W(VI) complexes, their preparation and use. More particularly, this invention relates to compounds of the formula WS(S.sub.2) (S.sub.2 CNR.sub.2).sub.2 which are mononuclear, seven-coordinate, neutral W(VI) complexes containing only seven sulfur atoms in the Mo coordination sphere. R is hydrogen, an alkyl, aryl, cycloalkyl group or mixture thereof. Preferably all of the R's are the same and are alkyl groups. These compounds are useful as catalysts or catalyst precursors for removing sulfur from sulfur containing hydrocarbons.

摘要翻译： 本发明涉及硫化（二硫化物）双（N，N-取代二硫代氨基甲酰基）W（Ⅵ）配合物及其制备和应用。 更具体地说，本发明涉及在Mo配位球中仅含有7个硫原子的单核，7位，中性W（VI）络合物的式WS（S2）（S2CNR2）2的化合物。 R是氢，烷基，芳基，环烷基或其混合物。 优选地，所有的R都是相同的并且是烷基。 这些化合物可用作从含硫烃中除去硫的催化剂或催化剂前体。

公开(公告)号：US5126465A

公开(公告)日：1992-06-30

申请号：US688212

申请日：1991-04-22

申请人： Mark A. Greaney ,  Catherine L. Coyle ,  Edward I. Stiefel

发明人： Mark A. Greaney ,  Catherine L. Coyle ,  Edward I. Stiefel

IPC分类号： C07F11/00

CPC分类号： C07F11/005

摘要： There is provided an improved method for preparing compounds of the formula Mo.sub.4 S.sub.4 L.sub.6 comprising:heating a solution of a compound having the formula MoL.sub.4, wherein L is a 1,1-dithioacid ligand, at a temperature and for a time sufficient to form the Mo.sub.4 S.sub.4 L.sub.6 compound. Preferably, the MoL.sub.4 compound is dissolved in an organic solvent and the solution is heated at temperatures above 25.degree. C., up to the boiling point of the solvent and, more preferably, at temperatures in the range of from about 50.degree. C. to about 250.degree. C.

摘要翻译： 提供了制备式Mo4S4L6化合物的改进方法，其包括：在足以形成Mo4S4L6化合物的温度和时间下，加热具有式MoL4的化合物（其中L为1,1-二硫酸配体）的溶液 。 优选地，将MoL 4化合物溶解在有机溶剂中，并将溶液在高于25℃的温度下加热至溶剂的沸点，更优选在约50℃至约50℃至 约250℃

公开(公告)号：US5110963A

公开(公告)日：1992-05-05

申请号：US708020

申请日：1991-05-24

申请人： Catherine L. Coyle ,  Scott A. Farina ,  Edward I. Stiefel ,  Mark A. Greaney

发明人： Catherine L. Coyle ,  Scott A. Farina ,  Edward I. Stiefel ,  Mark A. Greaney

IPC分类号： C07F11/00

CPC分类号： C07F11/005

摘要： The present invention is predicated on the discovery that Mo(III) containing compounds will react with salts of a 1,1-dithioacid to form Mo.sub.4 S.sub.4 L.sub.6. Accordingly, there is provided a method for preparing compounds of the formula Mo.sub.4 S.sub.4 L.sub.6 wherein L is a 1,1-dithioacid ligand comprising:contacting a Mo(III) containing compound with the salt of a 1,1-dithioacid at temperatures and for a time sufficient to form the Mo.sub.4 S.sub.4 L.sub.6 compound. Preferably, the Mo(III) containing compound is dissolved in an organic solvent and the solution is heated at temperatures above about 25.degree. C. up to the boiling point of the solvent and, preferably, at temperatures in the range of about 25.degree. C. to about 250.degree. C.

摘要翻译： 本发明基于以下发现：含有Mo（III）的化合物将与1,1-二硫酸的盐反应形成Mo 4 S 4 L 6。 因此，提供了制备式Mo 4 S 4 L 6的化合物的方法，其中L是1,1-二硫酸配体，其包括：使含Mo（III）的化合物与1,1-二硫酸的盐在温度和时间 足以形成Mo4S4L6化合物。 优选地，将含Mo（III）的化合物溶解在有机溶剂中，并将溶液在高于约25℃的温度下加热至溶剂的沸点，优选在约25℃的温度 至约250℃

公开(公告)号：US4997962A

公开(公告)日：1991-03-05

申请号：US202342

申请日：1988-06-06

申请人： Liwen Wei ,  Thomas R. Halbert ,  Edward I. Stiefel

发明人： Liwen Wei ,  Thomas R. Halbert ,  Edward I. Stiefel

IPC分类号： C01G47/00 ,  C07C211/62 ,  C07F13/00

CPC分类号： C01G47/006 ,  C07F13/005 ,  C01P2002/70 ,  C01P2002/80

摘要： According to the present invention, an improved method for preparing tetrathioperrhenate salts is provided. Basically, a water soluble, oxygen-containing rhenium compound such as rhenium oxide or a salt containing an oxyanion of rhenium, such as ReO.sub.4.sup.--, is contacted with an aqueous ammonium sulfide or polysulfide solution in the presence of a cation which is capable of forming an aqueous insoluble salt with tetrathioperrhenate.

公开(公告)号：US4995996A

公开(公告)日：1991-02-26

申请号：US450751

申请日：1989-12-14

申请人： Catherine L. Coyle ,  Mark A. Greaney ,  Edward I. Stiefel ,  James N. Francis ,  Morton Beltzer

发明人： Catherine L. Coyle ,  Mark A. Greaney ,  Edward I. Stiefel ,  James N. Francis ,  Morton Beltzer

IPC分类号： C10M135/14 ,  C10M159/18 ,  C10N10/12 ,  C10N20/02 ,  C10N30/06 ,  C10N30/12

CPC分类号： C10M159/18 ,  C10M135/14 ,  C10M2219/062 ,  C10N2210/06 ,  C10N2270/02

摘要： In accordance with this invention, there is provided a lubricating composition comprising a major amount of an oil of lubricating viscosity and a minor amount of an additive having the formula Mo.sub.2 L.sub.4 wherein L is a ligand selected from xanthates and mixtures thereof and, in particular, xanthates having a sufficient number of carbon atoms to render the additive soluble in the oil. In general, the xanthate ligand, L, will have form about 2 to 30 carbon atoms.

公开(公告)号：US4978464A

公开(公告)日：1990-12-18

申请号：US404143

申请日：1989-09-07

申请人： Catherine L. Coyle ,  Thomas R. Halbert ,  Edward I. Stiefel

发明人： Catherine L. Coyle ,  Thomas R. Halbert ,  Edward I. Stiefel

IPC分类号： C10M135/14 ,  C10M135/18 ,  C10M137/10 ,  C10M137/14 ,  C10M159/18 ,  C10N10/12 ,  C10N20/02 ,  C10N30/06 ,  C10N30/10

CPC分类号： C10M135/18 ,  C10M135/14 ,  C10M137/10 ,  C10M137/14 ,  C10M159/18 ,  C10M2219/062 ,  C10M2219/068 ,  C10M2223/045 ,  C10M2223/06 ,  C10M2223/061 ,  C10N2210/06 ,  C10N2270/02

摘要： A lubricating oil composition is provided which comprises a major amount of an oil of lubricating viscosity and a minor amount of an additive having the formula Mo.sub.4 S.sub.4 L.sub.6 in which L is a ligand selected from dithiocarbamates, dithiophosphates, dithiophosphinates, thioxanthates, and mixtures thereof and in which the ligands, L, have organo groups having a sufficient number of carbon atoms to render the additive soluble in the oil. In general, the organo groups of the ligands, L, will be the same, although they may be different and they preferably are selected from alkyl, aryl, substituted aryl and ether groups. For example, when L is a dialkyldithiocarbamate or a dialkyldithiophosphate, the alkyl groups will have from about 1 to 30 carbon atoms.